CN117772166A - Green and efficient regeneration method of active carbon in brine acidification-active carbon adsorption deodorization process - Google Patents
Green and efficient regeneration method of active carbon in brine acidification-active carbon adsorption deodorization process Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 628
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- 239000012267 brine Substances 0.000 title claims abstract description 109
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 title claims abstract description 109
- 238000011069 regeneration method Methods 0.000 title claims abstract description 98
- 238000000034 method Methods 0.000 title claims abstract description 74
- 230000008569 process Effects 0.000 title claims abstract description 38
- 238000004332 deodorization Methods 0.000 title claims abstract description 34
- 229910052799 carbon Inorganic materials 0.000 title abstract description 30
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims abstract description 74
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- 230000008929 regeneration Effects 0.000 claims abstract description 66
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- 239000002351 wastewater Substances 0.000 claims description 43
- 238000004519 manufacturing process Methods 0.000 claims description 38
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 150000003839 salts Chemical class 0.000 claims description 30
- 230000020477 pH reduction Effects 0.000 claims description 17
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- 238000005086 pumping Methods 0.000 claims description 12
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- 230000007935 neutral effect Effects 0.000 claims description 6
- 238000003860 storage Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 abstract description 19
- 231100000331 toxic Toxicity 0.000 abstract description 5
- 230000002588 toxic effect Effects 0.000 abstract description 5
- 230000004913 activation Effects 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 235000002639 sodium chloride Nutrition 0.000 description 33
- 229910052760 oxygen Inorganic materials 0.000 description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 15
- 239000001301 oxygen Substances 0.000 description 15
- 230000001877 deodorizing effect Effects 0.000 description 8
- 238000005342 ion exchange Methods 0.000 description 8
- 230000008901 benefit Effects 0.000 description 7
- 238000001228 spectrum Methods 0.000 description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 description 6
- 230000008859 change Effects 0.000 description 6
- 230000001172 regenerating effect Effects 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 5
- 230000001276 controlling effect Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 125000000524 functional group Chemical group 0.000 description 5
- 229910052740 iodine Inorganic materials 0.000 description 5
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- 238000011068 loading method Methods 0.000 description 4
- 230000035943 smell Effects 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 229910001919 chlorite Inorganic materials 0.000 description 3
- 229910052619 chlorite group Inorganic materials 0.000 description 3
- QBWCMBCROVPCKQ-UHFFFAOYSA-N chlorous acid Chemical compound OCl=O QBWCMBCROVPCKQ-UHFFFAOYSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 235000014113 dietary fatty acids Nutrition 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
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- 229930195729 fatty acid Natural products 0.000 description 3
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- CSJDCSCTVDEHRN-UHFFFAOYSA-N methane;molecular oxygen Chemical compound C.O=O CSJDCSCTVDEHRN-UHFFFAOYSA-N 0.000 description 3
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- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- -1 chlorine ions Chemical class 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 125000005842 heteroatom Chemical group 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
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- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 2
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- 241000894007 species Species 0.000 description 2
- XYHKNCXZYYTLRG-UHFFFAOYSA-N 1h-imidazole-2-carbaldehyde Chemical compound O=CC1=NC=CN1 XYHKNCXZYYTLRG-UHFFFAOYSA-N 0.000 description 1
- GWYFCOCPABKNJV-UHFFFAOYSA-M 3-Methylbutanoic acid Natural products CC(C)CC([O-])=O GWYFCOCPABKNJV-UHFFFAOYSA-M 0.000 description 1
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- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- OBOXTJCIIVUZEN-UHFFFAOYSA-N [C].[O] Chemical class [C].[O] OBOXTJCIIVUZEN-UHFFFAOYSA-N 0.000 description 1
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- GWYFCOCPABKNJV-UHFFFAOYSA-N beta-methyl-butyric acid Natural products CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 description 1
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- Treatment Of Water By Oxidation Or Reduction (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention discloses a green and efficient regeneration method of active carbon in a brine acidification-active carbon adsorption deodorization process, which is characterized by comprising the following steps of: s1, aeration, water washing and desalination; s2, ozone oxidation regeneration: adding alkali liquor with the same volume as the activated carbon into the activated carbon adsorption tower, blowing ozone from the bottom of the activated carbon adsorption tower so as to enable the ozone to perform oxidation reaction with the activated carbon under alkaline conditions, and then discharging waste alkali liquor; s3, washing out alkali by aeration water; s4, recycling waste liquid; s5, recycling the waste. The invention can avoid the loss of the activated carbon caused by high-temperature burning, has short regeneration and activation time, does not have harmful substance residues, and is very suitable for the regeneration of the activated carbon in the adsorption deodorization process of the acidified brine activated carbon; in addition, the waste liquid and the waste material in the active carbon regeneration process can be recycled, the whole process has no toxic and harmful waste emission, the method is green and environment-friendly, the treatment cost is low, the efficiency is high, and the method has better economy, environmental protection and feasibility.
Description
Technical Field
The invention relates to a regeneration method of active carbon, in particular to a green and efficient regeneration method of active carbon in a brine acidification-active carbon adsorption deodorization process.
Background
The productivity of Chinese crude salt reaches 1.2 hundred million tons, and most of the Chinese crude salt is used in chlor-alkali industry except common salt. China has become the largest chlor-alkali producing country and consumer country in the world at present. The primary salt production in the current stage of China mainly comprises sea salt, lake salt and well mineral salt. Wherein, the well mineral salt is gradually the main raw salt product due to higher quality. In the production of well mineral salt, the yield is highest in Sichuan province, and the quality is higher in Henan province. The future reserves of Henan salt-saving ore are 3500 hundred million tons, the content of ore grade sodium chloride is 75-90 percent, and the average content is more than 85 percent, belonging to caso4 type ore deposit. The content of harmful components and impurities in the Henan province salt field is low, and the national high-quality salt standard can be achieved. However, during the deposition and diagenesis of salt rock, the salt deposit contains a portion of residual organic matter, including short chain organic acid molecules and small amounts of hydrocarbon materials, which cause the brine and finished salt to be highly odorous. Therefore, in the salt production process, it is necessary to deodorize brine.
In the prior art, the relatively mature brine deodorization method comprises the following steps: a baking method, a redox method, a macroporous resin adsorption method and an aeration method. However, the above method still has some drawbacks, mainly represented by: the deodorizing effect is poor, the deodorizing agent is not friendly to the environment, and the deodorizing agent has the advantages of harmful substance residue, high deodorizing cost and the like. In order to solve the above problems, referring to fig. 1, the applicant proposes a method of acidifying brine, i.e. adding hydrochloric acid to the brine to adjust the pH to 3-5, and then using activated carbon for adsorption deodorization, wherein the adsorption capacity of activated carbon to brine can be greatly improved by acidifying brine. However, since the production profit of salt is very thin, and the amount of activated carbon used in brine deodorization is large, it is necessary to regenerate the deodorized activated carbon in order to reduce the production cost. At present, the regeneration method of the activated carbon mainly comprises the following steps:
1) Thermal regeneration method: the thermal regeneration method uses a gas such as steam, an inert gas, or carbon dioxide as an activating gas, and performs desorption analysis at a high temperature. The method has the advantages of no selectivity to the adsorbed substances and high regeneration efficiency. But has the defects of high heat regeneration temperature of 300-500 ℃, high energy consumption, and high active carbon consumption of 10% -20% on the other hand, and the method is unfavorable for reducing and controlling the production cost for the brine deodorization process with high active carbon consumption.
2) Chemical solvent regeneration method: the chemical solvent regeneration method utilizes the mutual balance relationship among the active carbon, the solvent and the absorbed matter, and the absorption matter is desorbed from the active carbon by changing the conditions of temperature, the pH value of the solvent and the like to break the balance. The method has the advantages of in-situ regeneration realization and lower cost. However, the method has the defects that the regeneration is not thorough, micropores are easy to block, the performance is obviously reduced after multiple regenerations, and especially the method has chemical solvent residues and can generate potential food safety hazards.
3) Biological regeneration method: the biological regeneration method relies on microorganisms propagated on activated carbon to oxidize and decompose the adsorbed organic substances to generate carbon dioxide and water, thereby recovering the adsorption performance. The method has the advantage of simplicity and easy implementation. However, the method has the defects that the method is greatly affected by water quality and temperature, intermediate products remain in the pores of the activated carbon, micropores are easily blocked, the regeneration is incomplete, and particularly, the regeneration time is too long, so that the method is difficult to be applied to salt-making industry of continuous operation.
In summary, the above-mentioned existing methods for regenerating activated carbon are difficult to be well adapted to the regeneration of activated carbon after deodorization of brine, so a new method for regenerating activated carbon applicable to the deodorization of brine needs to be researched and developed.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a green and efficient regeneration method of active carbon in a brine acidification-active carbon adsorption deodorization process, which can avoid active carbon loss caused by high-temperature burning, has short regeneration and activation time, does not have harmful substance residues, and is very suitable for the active carbon regeneration in the acidification brine active carbon adsorption deodorization process; in addition, the waste liquid and the waste material in the active carbon regeneration process can be recycled, the whole process has no toxic and harmful waste emission, and the method is green and environment-friendly, and has the advantages of low treatment cost, high efficiency, good economy, environmental protection and feasibility.
In order to achieve the above object, the present invention adopts the following technical scheme.
The green and efficient regeneration method of the activated carbon in the brine acidification-activated carbon adsorption deodorization process is characterized by comprising the following steps of:
s1, aeration, water washing and desalination: adding water with the same volume as the activated carbon into the activated carbon adsorption tower, blowing air from the bottom of the activated carbon adsorption tower, fully mixing the activated carbon with the water to remove salt in the activated carbon, and discharging the wastewater;
s2, ozone oxidation regeneration: adding alkali liquor with the same volume as the activated carbon into the activated carbon adsorption tower, blowing ozone from the bottom of the activated carbon adsorption tower so as to enable the ozone to perform oxidation reaction with the activated carbon under alkaline conditions, and then discharging waste alkali liquor;
s3, alkali is eluted by aeration water: adding water with the same volume as the activated carbon into the activated carbon adsorption tower, blowing air from the bottom of the activated carbon adsorption tower, fully mixing the activated carbon with the water to remove alkali liquor in the activated carbon, and discharging waste water to finish the regeneration of the activated carbon;
s4, recycling waste liquid: collecting the wastewater in the step S1, and directly pumping the wastewater into a brine production well for brine production; collecting the waste alkali liquor in the step S2 and the waste water in the step S3, merging and discharging the waste alkali liquor and the waste water into a waste liquid temporary storage tank, regulating the pH value of the merged waste liquid to be neutral, and then pumping the waste liquid into a brine production well for brine production;
s5, recycling waste materials: the activated carbon regenerated and used for a plurality of times in the steps S1, S2 and S3 is discharged into a boiler to be used as fuel for recycling;
in the brine acidification-activated carbon adsorption deodorization process, after the acidified brine is introduced into an activated carbon adsorption tower, the odor of the acidified brine cannot be adsorbed by activated carbon to be removed, namely, when the brine discharged from the activated carbon adsorption tower smells the odor, the activated carbon in the activated carbon adsorption tower is not suitable for deodorizing the brine in the next batch any more, and the activated carbon in the activated carbon adsorption tower needs to be subjected to the regeneration treatment at the moment;
in the step S1, the salt adsorbed by the activated carbon from the brine can be removed by aeration desalination, in particular to the chlorine ions in the activated carbon can be removed, so that the chlorine ions are prevented from being oxidized into chlorite, chlorate and other toxic and harmful substances by ozone in the next step, and the waste alkali liquor generated in the step S2 and the waste water generated in the step S3 can not be reused for washing the brine; because the activated carbon is used for adsorbing peculiar smell substances in brine, the peculiar smell substances are mainly low-grade fatty acids with 3-8 carbons, and part of gasoline substances such as short-chain alkane, and the like, the target components are complex, the water solubility is good, and especially the threshold value of the peculiar smell substances isovaleric acid is as low as 1.5ppm, the requirement on the adsorption performance of the activated carbon for deodorizing the brine is higher, so that the activated carbon regeneration is required to be more thorough; through the step S2, the activated carbon is regenerated under alkaline conditions, so that the oxidation capability of ozone can be improved, and 3-8 carbon lower fatty acids, and part of gasoline substances such as short-chain alkane and the like adsorbed by the activated carbon can be oxidized into carbon dioxide and water by utilizing the ozone, so that low-molecular-weight organic matters are rapidly oxidized, and the activated carbon can be regenerated in situ; because part of alkali liquor remains after the activated carbon is oxidized and regenerated by ozone, and the activated carbon is unfavorable for adsorbing and deodorizing the brine under the alkaline condition, the alkali is required to be eluted by aeration water in the step S3 so as to remove the alkali liquor in the activated carbon, thereby finally completing the regeneration of the activated carbon;
in the process, the wastewater in the step S1 contains salt, so that the wastewater can be directly pumped into a brine production well for brine production, so that rock salt in the brine production well is dissolved to form brine; the waste alkali liquor in the step S2 and the waste water in the step S3 contain alkali liquor and a small amount of ozone, and do not contain chlorite, chlorate and other toxic and harmful substances, and the ozone is rapidly decomposed in the placing process, so that the combined liquor of the alkali liquor and the ozone is returned to the pH value and can be used for halogen collection, and the zero emission of the waste liquor is realized by recycling the waste liquor generated in the steps S1-S3 for halogen collection; in addition, when the activated carbon is regenerated for a plurality of times in the steps S1 to S3, the activated carbon with serious attenuation of adsorption activity can be discharged into a boiler to be used as fuel after being dried at high temperature; therefore, the method of the invention not only can realize the regeneration of the activated carbon, but also can recycle the waste liquid and the waste material in the treatment process, has no waste discharge in the whole process, is friendly to the environment, and is beneficial to improving the comprehensive economic benefit of brine deodorization.
Preferably, in the steps S1 and S3, air is intermittently blown from the bottom of the activated carbon adsorption tower, and ultrasonic treatment is applied to the material in the activated carbon adsorption tower during the intermittent air blowing; in the steps S1 and S3, the salt and the residual alkali liquor in the activated carbon can be basically removed by repeated aeration water washing operation for a plurality of times, but the repeated operation for a plurality of times can increase the cost of manpower and material resources and generate a large amount of waste water and waste liquid; by combining ultrasonic waves, the effect of aeration washing can be greatly improved; however, air is blown into the bottom of the activated carbon adsorption tower during aeration water washing, and a large amount of air exists in the activated carbon adsorption tower, so that more cavities are formed in materials, the propagation of ultrasonic waves is affected, and the action effect of the ultrasonic waves is reduced; in contrast, according to the invention, air is intermittently blown from the bottom of the activated carbon adsorption tower, and ultrasonic treatment is applied to the material in the activated carbon adsorption tower during the intermittent period of air blowing, so that the combined effect of the air and the material can be exerted to the maximum extent, and the salt and residual alkali in the activated carbon can be removed by only one aeration water washing in the steps S1 and S3, and the operations of aeration water washing desalination and aeration water washing alkali removal are not required to be repeated, so that the treatment cost can be reduced and the activated carbon regeneration efficiency can be improved.
Preferably, in the steps S1 and S3, air is intermittently blown from the bottom of the activated carbon adsorption tower, that is, each time air is blown for 2-5 min, the air is intermittently blown for 1-2 min, and the total time of air blowing is controlled to be 20-30 min; ultrasonic treatment with the frequency of 25-60 kHz is applied to the material in the activated carbon adsorption tower during the intermittent period of air blowing.
Preferably, in the step S2, the alkali liquor is NaOH solution with the mass concentration of 0.01% -2.5%.
Preferably, in the step S2, the alkaline solution is NaOH solution with a mass concentration of 0.5%.
Preferably, in the step S2, the ozone inlet amount is 2-8 mg/L/min, and the ozone inlet time is 15-45 min.
Preferably, in the step S2, the ozone inlet amount is 5mg/L/min, and the ozone inlet time is 30min.
Preferably, in the step S2, the excessive ozone in the activated carbon adsorption tower is introduced into an ozone destruction device to be destroyed.
Preferably, in the step S5, the activated carbon regenerated and used for 7 times in the step S1 and the step S2 is discharged into a boiler to be reused as fuel.
Preferably, the activated carbon is wood activated carbon, and the granularity of the wood activated carbon is 30-50 meshes; the acidified brine is brine with pH value regulated to 3-5 by adding hydrochloric acid.
The beneficial effects of the invention are as follows:
1) Compared with the thermal regeneration method, the chemical solvent regeneration method and the biological regeneration method in the prior art, the invention adopts ozone to regenerate the active carbon under alkaline conditions, so that the active carbon loss caused by high-temperature burning can be avoided, the regeneration and activation time is short, harmful substance residues can not exist, and the method is very suitable for the active carbon regeneration in the adsorption deodorization process of the acidified brine active carbon; in addition, in the invention, the adsorption capacity of the activated carbon after 7 times of regeneration still can reach about 50% of the first use, namely, the activated carbon can be repeatedly used for 7 times by utilizing the method for regenerating the activated carbon, so that the use amount of the activated carbon in the adsorption deodorization production process of the brine activated carbon can be greatly reduced, and the economic benefit is remarkable especially for the salt production industry with slightly thin profit.
2) According to the invention, aeration water washing desalination is carried out before active carbon regeneration, so that chloride ions are prevented from being oxidized into chlorate, chlorite and other harmful substances by ozone, and thus, wastewater generated by aeration water washing desalination, waste lye generated by ozone oxidation regeneration and wastewater generated by aeration water washing alkali removal can be returned to a well for halogen production; meanwhile, after the activated carbon is regenerated for many times, the activated carbon with serious absorption activity attenuation can be discharged into a boiler to be used as fuel after being dried at high temperature; in summary, the method of the invention not only can realize the regeneration of the activated carbon, but also can recycle the waste liquid and the waste material in the treatment process, has no emission of toxic and harmful waste in the whole process, is environment-friendly, and has very low treatment cost, economical efficiency, environmental protection and feasibility.
Drawings
FIG. 1 is a flow chart of an acidified brine activated carbon adsorption deodorization process;
FIG. 2 is a graph of carbon-oxygen energy spectrum of activated carbon;
fig. 3 is an oxygen energy spectrum of activated carbon (arrows in the figure indicate the trend of change in binding energy of oxygen element).
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the present invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications could be made by those skilled in the art without departing from the inventive concept. These are all within the scope of the present invention.
Example 1
The green and efficient regeneration method of the activated carbon in the brine acidification-activated carbon adsorption deodorization process comprises the following steps:
s1, aeration, water washing and desalination: adding water with the same volume as the activated carbon into the activated carbon adsorption tower, blowing air from the bottom of the activated carbon adsorption tower, fully mixing the activated carbon with the water to remove salt in the activated carbon, discharging waste water, and repeating the operation for 1-3 times to ensure that the salt is removed completely;
s2, ozone oxidation regeneration: adding alkali liquor with the same volume as the activated carbon into the activated carbon adsorption tower, blowing ozone from the bottom of the activated carbon adsorption tower so as to enable the ozone to perform oxidation reaction with the activated carbon under alkaline conditions, and then discharging waste alkali liquor;
s3, alkali is eluted by aeration water: adding water with the same volume as the activated carbon into the activated carbon adsorption tower, blowing air from the bottom of the activated carbon adsorption tower to fully mix the activated carbon with the water to remove alkali liquor in the activated carbon, discharging waste water, and repeating the operation for 1-3 times to ensure that the residual alkali liquor is removed completely, thus finishing the regeneration of the activated carbon;
s4, recycling waste liquid: collecting the wastewater in the step S1, and directly pumping the wastewater into a brine production well for brine production; collecting the waste alkali liquor in the step S2 and the waste water in the step S3, merging and discharging the waste alkali liquor and the waste water into a waste liquid temporary storage tank, regulating the pH value of the merged waste liquid to be neutral, and then pumping the waste liquid into a brine production well for brine production;
s5, recycling the activated carbon: and (3) discharging the activated carbon regenerated and used for multiple times in the steps S1, S2 and S3 into a boiler to be used as fuel for recycling.
Example 2
The green and efficient regeneration method of the activated carbon in the brine acidification-activated carbon adsorption deodorization process comprises the following steps:
s1, aeration, water washing and desalination: adding water with the same volume as the activated carbon into the activated carbon adsorption tower, blowing air from the bottom of the activated carbon adsorption tower, fully mixing the activated carbon with the water to remove salt in the activated carbon, discharging waste water, and repeating the operation for 1-3 times to ensure that the salt is removed completely;
s2, ozone oxidation regeneration: adding alkali liquor with the same volume as the activated carbon into the activated carbon adsorption tower, blowing ozone from the bottom of the activated carbon adsorption tower so as to enable the ozone to perform oxidation reaction with the activated carbon under alkaline conditions, and then discharging waste alkali liquor; wherein the alkali liquor is NaOH solution with the mass concentration of 0.01% -2.5%; ozone is introduced into the reactor for 15-45 min at an ozone introducing amount of 2-8 mg/L/min; the excessive ozone in the activated carbon adsorption tower is introduced into an ozone destruction device for destruction;
s3, alkali is eluted by aeration water: adding water with the same volume as the activated carbon into the activated carbon adsorption tower, blowing air from the bottom of the activated carbon adsorption tower to fully mix the activated carbon with the water to remove alkali liquor in the activated carbon, discharging waste water, and repeating the operation for 1-3 times to ensure that the residual alkali liquor is removed completely, thus finishing the regeneration of the activated carbon;
s4, recycling waste liquid: collecting the wastewater in the step S1, and directly pumping the wastewater into a brine production well for brine production; collecting the waste alkali liquor in the step S2 and the waste water in the step S3, merging and discharging the waste alkali liquor and the waste water into a waste liquid temporary storage tank, regulating the pH value of the merged waste liquid to be neutral, and then pumping the waste liquid into a brine production well for brine production;
s5, recycling the activated carbon: and (3) drying the activated carbon regenerated and used for 7 times in the steps S1, S2 and S3, and discharging the dried activated carbon into a boiler to be used as fuel for recycling.
Example 3
The green and efficient regeneration method of the activated carbon in the brine acidification-activated carbon adsorption deodorization process comprises the following steps:
s1, aeration, water washing and desalination: adding water with the same volume as that of the activated carbon into an activated carbon adsorption tower, blowing air from the bottom of the activated carbon adsorption tower, controlling the time for blowing air to be 20-30 min, fully mixing the activated carbon with the water to remove salt in the activated carbon, discharging waste water, and repeating the operation for 2 times to ensure that the salt is removed completely;
s2, ozone oxidation regeneration: adding alkali liquor with the same volume as the activated carbon into the activated carbon adsorption tower, blowing ozone from the bottom of the activated carbon adsorption tower so as to enable the ozone to perform oxidation reaction with the activated carbon under alkaline conditions, and then discharging waste alkali liquor; wherein the alkali liquor is NaOH solution with the mass concentration of 0.5%; ozone is introduced into the reactor for 30min at an ozone introduction rate of 5 mg/L/min; the excessive ozone in the activated carbon adsorption tower is introduced into an ozone destruction device for destruction;
s3, alkali is eluted by aeration water: adding water with the same volume as the activated carbon into an activated carbon adsorption tower, blowing air from the bottom of the activated carbon adsorption tower, controlling the time of blowing air to be 20-30 min, fully mixing the activated carbon with the water to remove alkali liquor in the activated carbon, discharging waste water, and repeating the operation for 2 times to ensure that the residual alkali liquor is removed completely, thus finishing the regeneration of the activated carbon;
s4, recycling waste liquid: collecting the wastewater in the step S1, and directly pumping the wastewater into a brine production well for brine production; collecting the waste alkali liquor in the step S2 and the waste water in the step S3, merging and discharging the waste alkali liquor and the waste water into a waste liquid temporary storage tank, regulating the pH value of the merged waste liquid to be neutral, and then pumping the waste liquid into a brine production well for brine production;
s5, recycling the activated carbon: and (3) drying the activated carbon regenerated and used for 7 times in the steps S1, S2 and S3, and discharging the dried activated carbon into a boiler to be used as fuel for recycling.
Example 4
The green and efficient regeneration method of the activated carbon in the brine acidification-activated carbon adsorption deodorization process comprises the following steps:
s1, aeration, water washing and desalination: adding water with the same volume as that of the activated carbon into an activated carbon adsorption tower, intermittently blowing air from the bottom of the activated carbon adsorption tower, namely, intermittently blowing air for 2-5 min each time for 1-2 min, controlling the total time of blowing air to be 20-30 min, fully mixing the activated carbon with the water, applying ultrasonic treatment with the frequency of 25-60 kHz to the material in the activated carbon adsorption tower during the intermittent period of air blowing so as to remove salt in the activated carbon, and then discharging the waste water so as to ensure that the salt is removed completely;
s2, ozone oxidation regeneration: adding alkali liquor with the same volume as the activated carbon into the activated carbon adsorption tower, blowing ozone from the bottom of the activated carbon adsorption tower so as to enable the ozone to perform oxidation reaction with the activated carbon under alkaline conditions, and then discharging waste alkali liquor; wherein the alkali liquor is NaOH solution with the mass concentration of 0.5%; ozone is introduced into the reactor for 30min at an ozone introduction rate of 5 mg/L/min; the excessive ozone in the activated carbon adsorption tower is introduced into an ozone destruction device for destruction;
s3, alkali is eluted by aeration water: adding water with the same volume as the activated carbon into an activated carbon adsorption tower, intermittently blowing air from the bottom of the activated carbon adsorption tower, namely, intermittently blowing air for 2-5 min each time for 1-2 min, controlling the total time of blowing air to be 20-30 min, fully mixing the activated carbon with the water, applying ultrasonic treatment with the frequency of 25-60 kHz to the materials in the activated carbon adsorption tower during the intermittent period of air blowing so as to remove alkali liquor in the activated carbon, and then discharging waste water so as to ensure that residual alkali liquor is completely removed, thus finishing regeneration of the activated carbon;
s4, recycling waste liquid: collecting the wastewater in the step S1, and directly pumping the wastewater into a brine production well for brine production; collecting the waste alkali liquor in the step S2 and the waste water in the step S3, merging and discharging the waste alkali liquor and the waste water into a waste liquid temporary storage tank, regulating the pH value of the merged waste liquid to be neutral, and then pumping the waste liquid into a brine production well for brine production;
s5, recycling the activated carbon: drying the activated carbon regenerated and used for 7 times in the steps S1, S2 and S3, and discharging the dried activated carbon into a boiler to be used as fuel for recycling;
according to detection, the activated carbon is regenerated by adopting the steps S1-S3, the adsorption capacity of the activated carbon to brine is 2820, 2640 and 2310mg/L/min after the activated carbon is regenerated for 1-3 times, and compared with the data of the embodiment 8, the method can be used for desalting by aeration water washing, and the adsorption capacity of the regenerated activated carbon is not affected by intermittent air blowing and auxiliary ultrasonic treatment in the alkali-removing step of the aeration water washing, but the water washing operation is not required to be repeated in the steps S1 and S3, so that about one-fourth of the process time is saved, and the water consumption of water washing is greatly reduced.
Example 5
Inspection of ozone inlet amount in ozone oxidation regeneration.
1. Experimental method
Adding a proper amount of hydrochloric acid into brine, and uniformly stirring to adjust the pH of the brine to 3-5 to obtain acidified brine; loading 900-iodine value wood activated carbon with granularity of 30-50 meshes into an ion exchange column (in the embodiment, the ion exchange column is equivalent to an activated carbon adsorption tower) to obtain an activated carbon column; the acidified brine is passed through an activated carbon column, the airspeed is controlled to be 30-35L/h/kg, and the odor is smelled by the brine after passing through the column as the end point control, namely the activated carbon is required to be regenerated; at this time, the activated carbon in the column is regenerated by the method of steps S1 to S3 in example 3, and the parameters are different from those in example 3 in that in the control step S2, the ozone flow rates are respectively: 2mg/L/min, 5mg/L/min and 8mg/L/min, regenerating the activated carbon, and detecting the adsorption capacity of the regenerated activated carbon after different times. The adsorption capacity is controlled by the weight ratio of the acidified brine to the loaded activated carbon after passing through the column, and the odor is smelled after passing through the column.
2. Analysis of results
The results of examining the ozone introduction amount in the ozone oxidation regeneration are shown in Table 1.
TABLE 1 influence of ozone intake on adsorption Capacity after activated carbon regeneration
| Ozone inlet amount | 2mg/L/min | 5mg/L/min | 8mg/L/min |
| First use | 3000 | 3000 | 3000 |
| Regenerated 1 time | 2100 | 2850 | 2750 |
| Regenerated 2 times | 1200 | 2650 | 2260 |
| Regenerated 3 times | 500 | 2350 | 1650 |
As is clear from Table 1, when the ozone supply amount was 5mg/L/min for activated carbon regeneration, the adsorption capacity of the activated carbon after regeneration was maximized. Therefore, in the present invention, the ozone supply amount is preferably 5 mg/L/min.
Example 6
Inspection of ozone inlet time in ozone oxidation regeneration.
1. Experimental method
Adding a proper amount of hydrochloric acid into brine, and uniformly stirring to adjust the pH of the brine to 3-5 to obtain acidified brine; loading 900-iodine value wood activated carbon with granularity of 30-50 meshes into an ion exchange column (in the embodiment, the ion exchange column is equivalent to an activated carbon adsorption tower) to obtain an activated carbon column; the acidified brine is passed through an activated carbon column, the airspeed is controlled to be 30-35L/h/kg, and the odor is smelled by the brine after passing through the column as the end point control, namely the activated carbon is required to be regenerated; at this time, the activated carbon in the column is regenerated by the method of steps S1 to S3 in example 3, and the parameters are different from those in example 3 in that in the control step S2, the ozone flow rates are respectively: 15mg/L/min, 30mg/L/min and 45mg/L/min, regenerating the activated carbon, and detecting the adsorption capacity of the regenerated activated carbon after different times. The adsorption capacity is controlled by the weight ratio of the acidified brine to the loaded activated carbon after passing through the column, and the odor is smelled after passing through the column.
2. Analysis of results
The results of examining the ozone introduction time in the ozone oxidation regeneration are shown in Table 2.
TABLE 2 influence of ozone-on time on adsorption Capacity after activated carbon regeneration
| Ozone on time | 15min | 30min | 45min |
| First use | 3000 | 3000 | 3000 |
| Regenerated 1 time | 2200 | 2850 | 2820 |
| Regenerated 2 times | 1800 | 2650 | 2520 |
| Regenerated 3 times | 1750 | 2350 | 2150 |
As is clear from table 2, when the ozone on time is 20 minutes for activated carbon regeneration, the adsorption capacity of the activated carbon after regeneration is maximum. Therefore, in the present invention, the ozone supply time is preferably 30 mg/L/min.
Example 7
And (5) examining the concentration of alkali liquor in ozone oxidation regeneration.
1. Experimental method
Adding a proper amount of hydrochloric acid into brine, and uniformly stirring to adjust the pH of the brine to 3-5 to obtain acidified brine; loading 900-iodine value wood activated carbon with granularity of 30-50 meshes into an ion exchange column (in the embodiment, the ion exchange column is equivalent to an activated carbon adsorption tower) to obtain an activated carbon column; the acidified brine is passed through an activated carbon column, the airspeed is controlled to be 30-35L/h/kg, and the odor is smelled by the brine after passing through the column as the end point control, namely the activated carbon is required to be regenerated; at this time, the activated carbon in the column is regenerated by the method of steps S1 to S3 in example 3, and the difference from the parameters in example 3 is that in step S2, the mass concentrations of the alkali solution NaOH solution are respectively: 0.01%,0.5% and 2.5%, regenerating the activated carbon, and detecting the adsorption capacity of the regenerated activated carbon after different times. The adsorption capacity is controlled by the weight ratio of the acidified brine to the loaded activated carbon after passing through the column, and the odor is smelled after passing through the column.
2. Analysis of results
The results of examining the alkali concentration in the ozone oxidation regeneration are shown in Table 3.
TABLE 3 influence of lye concentration on adsorption Capacity after activated carbon regeneration
| Concentration of lye | 0.01％ | 0.5％ | 2.5％ |
| First use | 3000 | 3000 | 3000 |
| Regenerated 1 time | 2200 | 2850 | 2100 |
| Regenerated 2 times | 1600 | 2650 | 1650 |
| Regenerated 3 times | 1100 | 2350 | 1250 |
As is clear from Table 3, when the activated carbon was regenerated in 0.5% alkali solution, the adsorption capacity of the regenerated activated carbon was maximum. Therefore, in the present invention, the alkali concentration is preferably 0.5%.
Example 8
And (5) examining the regeneration times of the activated carbon.
1. Experimental method
1.1, an acidic brine activated carbon adsorption deodorization method comprises the following steps: adding a proper amount of hydrochloric acid into brine, and uniformly stirring to adjust the pH of the brine to 3-5 to obtain acidified brine; loading 900-iodine value wood activated carbon with granularity of 30-50 meshes into an ion exchange column (in the embodiment, the ion exchange column is equivalent to an activated carbon adsorption tower) to obtain an activated carbon column; the acidified brine is passed through an activated carbon column, the airspeed is controlled to be 30-35L/h/kg, and the odor is smelled by the brine after passing through the column as the end point control, namely the activated carbon is required to be regenerated;
1.2 activated carbon regeneration method: the activated carbon is regenerated by the method of steps S1-S3 in example 3, and after the activated carbon is regenerated, the activated carbon is continuously used for deodorizing the acidified brine according to the method of 1.1, and the adsorption capacity of the activated carbon on the brine under different times of regeneration is detected. The adsorption capacity is controlled by the weight ratio of the acidified brine to the loaded activated carbon after passing through the column, and the odor is smelled after passing through the column.
2. Analysis of results
TABLE 4 adsorption Capacity for activated carbon regeneration at different times
| Number of regenerations | Brine adsorption capacity |
| First use | 3000 |
| Regenerated 1 time | 2850 |
| Regenerated 2 times | 2650 |
| Regenerated 3 times | 2350 |
| Regenerated 4 times | 2150 |
| Regeneration 5 times | 1950 |
| Regenerated 6 times | 1700 |
| Regenerated 7 times | 1500 |
As is clear from Table 4, the activated carbon was regenerated by the method of the present invention, and the adsorption capacity of the activated carbon to brine gradually decreased as the number of times of regeneration increased, and after 7 times of regeneration, the adsorption capacity of the activated carbon was about 50% of the first adsorption capacity, and thus the method still had a practical value. The activated carbon is continuously regenerated, the adsorption activity attenuation is serious, the adsorption capacity is reduced to below 50% of the first adsorption capacity, when the adsorption capacity of the regenerated activated carbon is too low, the frequency of the regeneration of the activated carbon is increased, the production is further influenced, and the production cost is increased, so that the activated carbon is not continuously used after being regenerated for 7 times. At the moment, the activated carbon can be discharged into a boiler to be used as fuel after being dried at high temperature, and waste pollution and resource waste are avoided.
Example 9
The method of the invention regenerates the influence of the activated carbon on the oxygen-containing functional group of the activated carbon.
The oxygen-containing functional groups on the surface of the activated carbon can change the properties and the behaviors of the surface of the activated carbon, thereby leading to the change of the adsorption performance of the activated carbon on organic matters. In the embodiment, XPS energy spectrum is adopted to examine the number and valence changes of oxygen atoms of oxygen-containing functional groups on the surface of the activated carbon.
1. Experimental method
The method is characterized in that 900 iodine value, unused wood activated carbon with granularity of 30-50 meshes and activated carbon regenerated for 1 time and 7 times in the embodiment 8 are taken as detection objects, an XPS full spectrum and C, O fine spectrum of the three are detected by adopting a Thermo Fisher Scientific Escalab xi +X-ray photoelectron spectrometer, and the carbon-oxygen ratio change in the activated carbon regeneration process is calculated, and the results are shown in fig. 2, fig. 3 and Table 5, wherein fig. 2 is a carbon-oxygen spectrum of the three, and fig. 3 is an oxygen spectrum of the three.
2. Analysis of results
TABLE 5 variation of carbon to oxygen ratio during regeneration of activated carbon
| Sample of | Oxygen atom ratio/% | Carbon atom ratio/% |
| Unused activated carbon | 12.63 | 87.37 |
| Activated carbon is regenerated 1 time | 12.46 | 87.54 |
| Activated carbon is regenerated 7 times | 12.46 | 87.54 |
As can be seen from fig. 2, the surface of the unused activated carbon is mainly carbon, and oxygen is two elements, which indicates that the activated carbon is basically not doped with other hetero elements, and the activated carbon after 1 time and 7 times of regeneration is basically not introduced with hetero atoms. In order to investigate the change of the oxygen-containing species on the surface of the activated carbon after use, it is known from fig. 3 that the combination energy of oxygen elements moves toward a lower valence state after 1 time of regeneration of the activated carbon, which indicates that a small amount of the oxygen-containing species on the surface of the activated carbon is reduced after 1 time of regeneration, and when the activated carbon is regenerated 7 times, it can be seen that the oxygen species on the surface of the activated carbon is obviously reduced. As is clear from table 5, by comparing the oxygen atom ratios of the three activated carbon oxygen samples, the oxygen atom content of the oxygen-containing functional groups on the activated carbon surface was slightly reduced after the activated carbon was oxidized and regenerated 1 time, but the oxygen atom content of both the regeneration times and the regeneration times were unchanged from each other compared with each other by 7 times, which indicates that the cause of the reduction in the adsorption capacity of the activated carbon to the odor substances such as the lower fatty acids was not the reduction in the oxygen-containing functional groups, but the reduction in the adsorption capacity due to the change in the valence state of the oxygen element was possible.
Claims (10)
1. The green and efficient regeneration method of the activated carbon in the brine acidification-activated carbon adsorption deodorization process is characterized by comprising the following steps of:
s1, aeration, water washing and desalination: adding water with the same volume as the activated carbon into the activated carbon adsorption tower, blowing air from the bottom of the activated carbon adsorption tower, fully mixing the activated carbon with the water to remove salt in the activated carbon, and discharging the wastewater;
s2, ozone oxidation regeneration: adding alkali liquor with the same volume as the activated carbon into the activated carbon adsorption tower, blowing ozone from the bottom of the activated carbon adsorption tower so as to enable the ozone to perform oxidation reaction with the activated carbon under alkaline conditions, and then discharging waste alkali liquor;
s3, alkali is eluted by aeration water: adding water with the same volume as the activated carbon into the activated carbon adsorption tower, blowing air from the bottom of the activated carbon adsorption tower, fully mixing the activated carbon with the water to remove alkali liquor in the activated carbon, and discharging waste water to finish the regeneration of the activated carbon;
s4, recycling waste liquid: collecting the wastewater in the step S1, and directly pumping the wastewater into a brine production well for brine production; collecting the waste alkali liquor in the step S2 and the waste water in the step S3, merging and discharging the waste alkali liquor and the waste water into a waste liquid temporary storage tank, regulating the pH value of the merged waste liquid to be neutral, and then pumping the waste liquid into a brine production well for brine production;
s5, recycling the activated carbon: and (3) discharging the activated carbon regenerated and used for a plurality of times through the steps S1 to S3 into a boiler to be reused as fuel.
2. The green and efficient regeneration method for activated carbon in a brine acidification-activated carbon adsorption deodorization process according to claim 1, wherein in the steps S1 and S3, air is intermittently blown from the bottom of the activated carbon adsorption tower, and ultrasonic treatment is applied to the material in the activated carbon adsorption tower during the intermittent air blowing.
3. The green and efficient regeneration method of the activated carbon in the brine acidification-activated carbon adsorption deodorization process according to claim 2, wherein in the steps S1 and S3, air is intermittently blown from the bottom of the activated carbon adsorption tower, namely, every 2-5 min, the air is intermittently blown for 1-2 min, and the total time of blowing air is controlled to be 20-30 min; ultrasonic treatment with the frequency of 25-60 kHz is applied to the material in the activated carbon adsorption tower during the intermittent period of air blowing.
4. The green and efficient regeneration method of the activated carbon in the brine acidification-activated carbon adsorption deodorization process of claim 1, wherein in the step S2, the alkali liquor is NaOH solution with the mass concentration of 0.01% -2.5%.
5. The green and efficient regeneration method of activated carbon in a brine acidification-activated carbon adsorption deodorization process according to claim 4, wherein in the step S2, the alkali liquor is a NaOH solution with a mass concentration of 0.5%.
6. The green and efficient regeneration method of the activated carbon in the brine acidification-activated carbon adsorption deodorization process according to claim 1, wherein in the step S2, the ozone inlet amount is 2-8 mg/L/min, and the ozone inlet time is 15-45 min.
7. The green and efficient regeneration method of activated carbon in a brine acidification-activated carbon adsorption deodorization process according to claim 6, wherein in the step S2, the ozone inlet amount is 5mg/L/min, and the ozone inlet time is 30min.
8. The green and efficient regeneration method of activated carbon in a brine acidification-activated carbon adsorption deodorization process according to claim 1, wherein in the step S2, excessive ozone in an activated carbon adsorption tower is introduced into an ozone destruction device for destruction.
9. The green and efficient regeneration method of the activated carbon in the brine acidification-activated carbon adsorption deodorization process of claim 1, wherein in the step S5, the activated carbon regenerated in the step S1 and the step S2 for 7 times is discharged into a boiler to be used as fuel for recycling.
10. The green and efficient regeneration method of the activated carbon in the brine acidification-activated carbon adsorption deodorization process of claim 1, wherein the activated carbon is wood activated carbon with the granularity of 30-50 meshes; the acidified brine is brine with pH value regulated to 3-5 by adding hydrochloric acid.
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